Method for producing solid electrolyte having argyrodite type crystal structure

a technology of argyrodite and crystal structure, which is applied in the direction of electrolytes, cell components, electrical equipment, etc., can solve the problems of inability to produce batteries, short circuits, and inability to obtain fine solid electrolyte suitable for solid electrolyte layers having a thickness on the order of submicron,

Active Publication Date: 2022-07-05
IDEMITSU KOSAN CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Benefits of technology

[0016]In addition, when the heat treatment is performed at a low temperature in order to suppress the growth of particles, there has been a problem that impurities such as unreacted raw materials tend to remain in the solid electrolyte. LiBr also remains in the solid electrolyte obtained by the method of Non-Patent Document 2. The presence of the residual raw material may reduce the ionic conductivity. In addition, since lithium halide absorbs water, the water-resistance of the solid electrolyte may be lowered.
[0017]An object of the present invention is to provide a method for producing an argyrodite-type solid electrolyte having a small particle size and a high ionic conductivity, and having a less amount of the residual raw material.
[0022]According to an embodiment of the present invention, it is possible to provide a method for producing an argyrodite-type solid electrolyte having a small particle size and a high ionic conductivity, and having a less amount of the residual raw material.

Problems solved by technology

In the conventional producing method including the step of heat treatment at a high temperature, particles grow large, and therefore, for example, a fine solid electrolyte suitable for a solid electrolyte layer having a thickness on the order of submicron cannot be obtained.
For example, if the particles of the solid electrolyte become coarse at the time of production or use of the battery, a short circuit is caused.
In some cases, the battery itself cannot be produced.
In addition, when the heat treatment is performed at a low temperature in order to suppress the growth of particles, there has been a problem that impurities such as unreacted raw materials tend to remain in the solid electrolyte.
The presence of the residual raw material may reduce the ionic conductivity.

Method used

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  • Method for producing solid electrolyte having argyrodite type crystal structure
  • Method for producing solid electrolyte having argyrodite type crystal structure
  • Method for producing solid electrolyte having argyrodite type crystal structure

Examples

Experimental program
Comparison scheme
Effect test

production example 1

Production of Lithium Sulfide (Li2S)

[0122]Li2S was produced and purified as described below.

[0123]As a water-insoluble medium, toluene (manufactured by Sumitomo Corporation) was dehydrated, and 303.8 kg of toluene having a moisture content of 100 ppm, which was measured by a Karl Fisher moisture meter, was added to a 500 L reaction kiln made of stainless steel under a nitrogen stream. Then, 33.8 kg of anhydrous lithium hydroxide (manufactured by Honjo Chemical Co., Ltd.) was addition, and the mixture was kept at 95° C. while being stirred at 131 rpm by a twin star stirring blade.

[0124]Hydrogen sulfide (manufactured by Sumitomo Seika Co., Ltd.) was blown into the slurry at a feed rate of 100 L / min, and the temperature was raised to 104° C. An azeotropic gas of water and toluene was continuously discharged from the reaction kiln. This azeotropic gas was condensed by an out-of-system condenser to achieve dehydration. In the meantime, the same amount of toluene as distilling toluene was...

example 1

(A) Pulverizing Step

[0128]Li2S obtained in Production Example 1 was pulverized in a nitrogen atmosphere using a pin mill (100UPZ manufactured by Hosokawa Micron Co., Ltd.) having a fixed quantity machine. The addition rate was 80 g / min, and the rotation speed of the disk was 18000 rpm.

[0129]Similarly, P2S5 (manufactured by Thermophos, laser diffraction D50=125 μm), LiBr (manufactured by Honjo Chemical, laser diffraction D50=38 μm), and LiCl (manufactured by Sigma Aldrich, laser diffraction D50=308 μm) were each pulverized by a pin mill. The addition rate of P2S5 was 140 g / min, the addition rate of LiBr was 230 g / min, and the addition rate of LiCl was 250 g / min. The rotation speed of each disk was 18000 rpm.

[0130]The laser diffraction D50 of Li2S after pulverizing was 7.7 μm, the laser diffraction D50 of P2S5 after pulverizing was 8.7 μm, the laser diffraction D50 of LiBr after pulverizing was 5.0 μm, and the laser diffraction D50 of LiCl after pulverizing was 10 μm, respectively.

(B)...

example 2

[0141]In Example 1(B), the slurry after treatment with the bead mill was used in the heat-treating step without drying. The slurry was put into an autoclave and heat-treated at 180° C. for 2 hours. Except for the foregoing, a solid electrolyte was produced and evaluated in the same manner as in Example 1. The results are shown in Tables 1 and 2.

[0142]The XRD pattern of the treated product is shown in FIG. 3. The XRD pattern of the solid electrolyte is shown in FIG. 4.

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Abstract

A method for producing a solid electrolyte having an argyrodite-type crystal structure, the method comprising:heat-treating a raw material mixture comprising lithium, sulfur, phosphorus and halogen in a solvent using a pressure-resistant container or under refluxing;removing the solvent; andfiring a treated product obtained by the heat treatment.

Description

TECHNICAL FIELD[0001]The embodiments described in the present specification relates generally to a method for producing a solid electrolyte having an argyrodite-type crystal structure.BACKGROUND ART[0002]With the rapid spread of information-related equipments or communications equipments such as personal computers, video cameras, and mobile phones in recent years, the development of batteries used as a power source thereof has been considered to be important. Among these batteries, a lithium ion battery has attracted an attention in terms of its high energy density.[0003]In the lithium ion battery that is currently commercially available, a liquid electrolyte containing a flammable organic solvent is used, and therefore, it is required to attach of a safety device that suppresses an increase of a temperature at the time of short circuit, or to make improvements in structural and material aspects for preventing short circuit. On the other hand, in the lithium ion battery formed into ...

Claims

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Application Information

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Patent Type & Authority Patents(United States)
IPC IPC(8): H01M10/0562H01M10/0525
CPCH01M10/0562H01M10/0525H01M2300/008H01M2300/0068
Inventor MASUDA, NAOYAMARUYAMA, JUNPEIKIMPARA, HIRONARITOTSUKA, SHOTAYAO, ATSUSHI
Owner IDEMITSU KOSAN CO LTD
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